Phosphoric Acid → HCID 5362051、化合物

HRID 1493437

反応式

HRID 1493437 の反応式
[CH3:1][C:2]([O:7]/[N:8]=[C:9](\[C:16]([NH:18][C@@H:19]1[C:22](=[O:23])[N:21]2[C:24]([C:35]([O-:37])=[O:36])=[C:25]([CH2:28][N+:29]3[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=3)[CH2:26][S:27][C@H:20]12)=[O:17])/[C:10]1[N:14]=[C:13]([NH2:15])[S:12][CH:11]=1)([C:4]([OH:6])=[O:5])[CH3:3].P(=O)(O)(O)[OH:39]>>[CH3:3][C:2]([O:7]/[N:8]=[C:9](/[C:16]([NH:18][C@@H:19]1[C:22](=[O:23])[N:21]2[C:24]([C:35]([O-:37])=[O:36])=[C:25]([CH2:28][N+:29]3[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=3)[CH2:26][S:27][C@H:20]12)=[O:17])\[C:10]1[N:14]=[C:13]([NH2:15])[S:12][CH:11]=1)([C:4]([OH:6])=[O:5])[CH3:1].[OH2:39].[OH2:5].[OH2:5].[OH2:5].[OH2:5]

参加物

3

反応物 2

HCID 1004Phosphoric Acid2 回HCID 5481173Ceftazidime

生成物 1

HCID 5362051HCID 5362051、化合物収率 77.3%

反応条件

温度
2.5 °C

実験手順

The pH of the ceftazidime solution was lowered to 4.5 with 4M phosphoric acid, and the solution was seeded. The solution was stirred for 21/2 hr at 0-5° C., during which the pH had risen to 4.7 and a large amount of crystals had formed. Phosphoric acid (4M) was then added dropwise over a 1 hr period to achieve a pH of 3.7. More acid was added dropwise over the next 1/2 hr to maintain this pH. After the pH was stabilized, the slurry was stirred slowly in an ice bath for 1 hr. The crystals were filtered and washed twice with cold deionized water (2×30 mL) and then with cold acetone (30 mL). The product was dried overnight at ambient temperature at a pressure of about 80 mm Hg. This procedure gave 13.57 g of ceftazidime pentahydrate. The assay was 85.4%, and the corrected yield was 77.3%. Another 11.1% yield was obtained from the combined mother liquors and washes.

後処理

  1. customa large amount of crystals had formed
  2. additionMore acid was added dropwise over the next 1/2 hr
  3. temperatureto maintain this pH
  4. stirringthe slurry was stirred slowly in an ice bath for 1 hr
  5. filtrationThe crystals were filtered
  6. washwashed twice with cold deionized water (2×30 mL)
  7. customThe product was dried overnight at ambient temperature at a pressure of about 80 mm Hg

出典と根拠

ORDレコード
ord-8e4e06a4982d40d5989a781ce58dbdca
出典データセット
uspto-grants-1991_06
特許番号
US05021564

関連ノート

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